#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:29:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179113 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/75/4307597.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4307597
loop_
_publ_author_name
'Guillem Aromí'
'Patrick Gamez'
'J. Krzystek'
'Huub Kooijman'
'Anthony L. Spek'
'Elizabeth J. MacLean'
'Simon J. Teat'
'Harriott Nowell'
_publ_contact_author_address
;   Bijvoet Center for Biomolecular Research
    Crystal and Structural Chemistry
    Utrecht University
    Padualaan 8
    3584 CH Utrecht
    The Netherlands
;
_publ_contact_author_email       h.kooijman@chem.uu.nl
_publ_contact_author_fax         '+31 30 2533940'
_publ_contact_author_name        '   Dr. H. Kooijman'
_publ_contact_author_phone       '+31 30 2532533'
_publ_section_title
;
Novel Linear Transition Metal Clusters of a Heptadentate Bis-β-diketone
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2519
_journal_page_last               2529
_journal_paper_doi               10.1021/ic062075v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C39 H28 Co N3 O7'
_chemical_formula_weight         709.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.615(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.932(2)
_cell_length_b                   9.0376(17)
_cell_length_c                   28.463(5)
_cell_measurement_reflns_used    2065
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.780
_cell_measurement_theta_min      3.708
_cell_volume                     3323.1(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs''
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2SMX'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.84640
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18576
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         3.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.9543
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0543P)²+2.4756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                3855
_reflns_number_total             4937
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic062075vsi20061030_124021_4.cif
_cod_data_source_block           2
_cod_database_code               4307597
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.34245(3) 0.42241(5) 0.111134(16) 0.01724(17) Uani 1 1 d . . .
O1 O 0.1735(2) 0.5506(3) 0.22858(9) 0.0341(7) Uani 1 1 d . . .
O2 O 0.29357(18) 0.5609(2) 0.16217(8) 0.0213(6) Uani 1 1 d . . .
O3 O 0.45134(18) 0.5810(2) 0.09980(8) 0.0210(6) Uani 1 1 d . . .
O4 O 0.5489(2) 0.6167(3) 0.02625(9) 0.0322(7) Uani 1 1 d . . .
O5 O 0.60649(17) 0.7071(2) -0.05953(8) 0.0194(6) Uani 1 1 d . . .
O6 O 0.77437(17) 0.7280(3) -0.12023(8) 0.0201(6) Uani 1 1 d . . .
O7 O 0.95184(19) 0.6798(3) -0.15177(9) 0.0294(6) Uani 1 1 d . . .
C20 C 0.2960(3) 0.7047(4) 0.16059(12) 0.0196(8) Uani 1 1 d . . .
C21 C 0.2218(3) 0.7807(4) 0.19110(12) 0.0200(8) Uani 1 1 d . . .
C22 C 0.1643(3) 0.7004(4) 0.22345(12) 0.0219(8) Uani 1 1 d . . .
C23 C 0.0964(3) 0.7737(4) 0.25225(12) 0.0250(9) Uani 1 1 d . . .
H23 H 0.0582 0.7184 0.2739 0.030 Uiso 1 1 calc R . .
C24 C 0.0840(3) 0.9239(4) 0.24969(13) 0.0286(9) Uani 1 1 d . . .
H24 H 0.0381 0.9726 0.2697 0.034 Uiso 1 1 calc R . .
C25 C 0.1390(3) 1.0048(4) 0.21757(13) 0.0305(10) Uani 1 1 d . . .
H25 H 0.1302 1.1090 0.2154 0.037 Uiso 1 1 calc R . .
C26 C 0.2058(3) 0.9345(4) 0.18908(13) 0.0269(9) Uani 1 1 d . . .
H26 H 0.2425 0.9913 0.1672 0.032 Uiso 1 1 calc R . .
C30 C 0.4382(3) 0.7216(4) 0.10470(12) 0.0193(8) Uani 1 1 d . . .
C31 C 0.3640(3) 0.7831(4) 0.13317(12) 0.0226(8) Uani 1 1 d . . .
H31 H 0.3594 0.8880 0.1339 0.027 Uiso 1 1 calc R . .
C40 C 0.5573(3) 0.7611(4) 0.03799(12) 0.0197(8) Uani 1 1 d . . .
C41 C 0.6167(3) 0.8537(4) 0.00968(12) 0.0180(8) Uani 1 1 d . . .
C42 C 0.5076(3) 0.8190(4) 0.07732(12) 0.0207(8) Uani 1 1 d . . .
C43 C 0.6302(3) 1.0001(4) 0.02280(13) 0.0226(9) Uani 1 1 d . . .
H43 H 0.6711 1.0627 0.0043 0.027 Uiso 1 1 calc R . .
C44 C 0.5244(3) 0.9682(4) 0.08896(12) 0.0217(8) Uani 1 1 d . . .
H44 H 0.4930 1.0084 0.1157 0.026 Uiso 1 1 calc R . .
C45 C 0.5855(3) 1.0580(4) 0.06246(12) 0.0228(8) Uani 1 1 d . . .
H45 H 0.5970 1.1583 0.0712 0.027 Uiso 1 1 calc R . .
C50 C 0.6614(3) 0.7968(4) -0.03465(12) 0.0198(8) Uani 1 1 d . . .
C51 C 0.7611(3) 0.8468(4) -0.04602(12) 0.0211(8) Uani 1 1 d . . .
H51 H 0.7959 0.9109 -0.0241 0.025 Uiso 1 1 calc R . .
C60 C 0.8129(3) 0.8108(4) -0.08636(12) 0.0197(8) Uani 1 1 d . . .
C61 C 0.9215(3) 0.8639(4) -0.09173(12) 0.0192(8) Uani 1 1 d . . .
C62 C 0.9869(3) 0.7910(4) -0.12305(12) 0.0231(8) Uani 1 1 d . . .
C63 C 1.0909(3) 0.8317(4) -0.12416(13) 0.0301(10) Uani 1 1 d . . .
H63 H 1.1355 0.7786 -0.1437 0.036 Uiso 1 1 calc R . .
C64 C 1.1296(3) 0.9468(4) -0.09746(13) 0.0309(10) Uani 1 1 d . . .
H64 H 1.2003 0.9740 -0.0990 0.037 Uiso 1 1 calc R . .
C65 C 1.0659(3) 1.0237(4) -0.06818(13) 0.0299(9) Uani 1 1 d . . .
H65 H 1.0923 1.1047 -0.0501 0.036 Uiso 1 1 calc R . .
C66 C 0.9639(3) 0.9818(4) -0.06552(13) 0.0247(9) Uani 1 1 d . . .
H66 H 0.9209 1.0348 -0.0452 0.030 Uiso 1 1 calc R . .
N70 N 0.4420(2) 0.3091(3) 0.16280(10) 0.0222(7) Uani 1 1 d . . .
C71 C 0.5460(3) 0.3169(4) 0.16172(14) 0.0309(10) Uani 1 1 d . . .
H71 H 0.5757 0.3772 0.1386 0.037 Uiso 1 1 calc R . .
C72 C 0.6102(3) 0.2413(5) 0.19273(16) 0.0458(12) Uani 1 1 d . . .
H72 H 0.6831 0.2510 0.1913 0.055 Uiso 1 1 calc R . .
C73 C 0.5688(4) 0.1507(5) 0.22617(16) 0.0482(12) Uani 1 1 d . . .
H73 H 0.6124 0.0956 0.2475 0.058 Uiso 1 1 calc R . .
C74 C 0.4630(4) 0.1423(5) 0.22774(15) 0.0463(12) Uani 1 1 d . . .
H74 H 0.4316 0.0815 0.2503 0.056 Uiso 1 1 calc R . .
C75 C 0.4031(3) 0.2243(4) 0.19581(14) 0.0321(10) Uani 1 1 d . . .
H75 H 0.3300 0.2198 0.1975 0.039 Uiso 1 1 calc R . .
N80 N 0.2373(2) 0.5372(3) 0.06020(10) 0.0211(7) Uani 1 1 d . . .
C81 C 0.1396(3) 0.5703(4) 0.07012(13) 0.0262(9) Uani 1 1 d . . .
H81 H 0.1175 0.5499 0.1008 0.031 Uiso 1 1 calc R . .
C82 C 0.0702(3) 0.6320(4) 0.03812(14) 0.0331(10) Uani 1 1 d . . .
H82 H 0.0013 0.6521 0.0464 0.040 Uiso 1 1 calc R . .
C83 C 0.1018(3) 0.6647(4) -0.00644(15) 0.0353(10) Uani 1 1 d . . .
H83 H 0.0555 0.7090 -0.0292 0.042 Uiso 1 1 calc R . .
C84 C 0.2018(3) 0.6317(4) -0.01712(14) 0.0355(10) Uani 1 1 d . . .
H84 H 0.2256 0.6516 -0.0476 0.043 Uiso 1 1 calc R . .
C85 C 0.2669(3) 0.5695(4) 0.01692(13) 0.0273(9) Uani 1 1 d . . .
H85 H 0.3362 0.5484 0.0094 0.033 Uiso 1 1 calc R . .
N1S N 0.1486(4) 0.0792(5) 0.36681(16) 0.0710(13) Uani 1 1 d . . .
C2S C 0.0988(3) 0.1970(5) 0.34296(15) 0.0427(11) Uani 1 1 d . . .
H2S H 0.0260 0.2094 0.3442 0.051 Uiso 1 1 calc R . .
C3S C 0.1558(4) 0.2934(5) 0.31802(16) 0.0449(12) Uani 1 1 d . . .
H3S H 0.1237 0.3735 0.3014 0.054 Uiso 1 1 calc R . .
C4S C 0.2611(4) 0.2720(5) 0.31737(17) 0.0519(13) Uani 1 1 d . . .
H4S H 0.3035 0.3381 0.3009 0.062 Uiso 1 1 calc R . .
C5S C 0.3034(4) 0.1524(6) 0.34122(18) 0.0532(13) Uani 1 1 d . . .
H5S H 0.3761 0.1381 0.3404 0.064 Uiso 1 1 calc R . .
C6S C 0.2501(3) 0.0572(4) 0.36490(15) 0.0331(10) Uani 1 1 d . . .
H6S H 0.2828 -0.0249 0.3802 0.040 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O3 85.43(9) . . ?
O2 Co1 O5 177.64(9) . 3_665 ?
O2 Co1 O6 93.60(9) . 3_665 ?
O2 Co1 N70 90.04(10) . . ?
O2 Co1 N80 88.72(10) . . ?
O3 Co1 O5 92.36(9) . 3_665 ?
O3 Co1 O6 176.13(10) . 3_665 ?
O3 Co1 N70 92.63(10) . . ?
O3 Co1 N80 88.58(10) . . ?
O5 Co1 O6 88.55(9) 3_665 3_665 ?
O5 Co1 N70 90.90(10) 3_665 . ?
O5 Co1 N80 90.39(10) 3_665 . ?
O6 Co1 N70 91.11(10) 3_665 . ?
O6 Co1 N80 87.65(10) 3_665 . ?
N70 Co1 N80 178.19(11) . . ?
Co1 O2 C20 125.4(2) . . ?
Co1 O3 C30 125.3(2) . . ?
Co1 O5 C50 125.7(2) 3_665 . ?
Co1 O6 C60 123.0(2) 3_665 . ?
O2 C20 C21 115.0(3) . . ?
O2 C20 C31 122.9(3) . . ?
C21 C20 C31 122.0(3) . . ?
C20 C21 C22 121.1(3) . . ?
C20 C21 C26 121.9(3) . . ?
C22 C21 C26 117.0(3) . . ?
O1 C22 C21 122.2(3) . . ?
O1 C22 C23 117.5(3) . . ?
C21 C22 C23 120.3(3) . . ?
C22 C23 C24 121.0(3) . . ?
C23 C24 C25 119.6(3) . . ?
C24 C25 C26 120.1(4) . . ?
C21 C26 C25 122.1(3) . . ?
O3 C30 C31 123.4(3) . . ?
O3 C30 C42 115.9(3) . . ?
C31 C30 C42 120.7(3) . . ?
C20 C31 C30 126.1(3) . . ?
O4 C40 C41 118.1(3) . . ?
O4 C40 C42 121.2(3) . . ?
C41 C40 C42 120.7(3) . . ?
C40 C41 C43 118.5(3) . . ?
C40 C41 C50 121.1(3) . . ?
C43 C41 C50 120.3(3) . . ?
C30 C42 C40 119.9(3) . . ?
C30 C42 C44 122.1(3) . . ?
C40 C42 C44 118.0(3) . . ?
C41 C43 C45 121.7(3) . . ?
C42 C44 C45 121.5(3) . . ?
C43 C45 C44 119.4(3) . . ?
O5 C50 C41 117.4(3) . . ?
O5 C50 C51 124.5(3) . . ?
C41 C50 C51 118.1(3) . . ?
C50 C51 C60 126.1(3) . . ?
O6 C60 C51 124.2(3) . . ?
O6 C60 C61 115.9(3) . . ?
C51 C60 C61 119.8(3) . . ?
C60 C61 C62 120.3(3) . . ?
C60 C61 C66 122.4(3) . . ?
C62 C61 C66 117.3(3) . . ?
O7 C62 C61 121.9(3) . . ?
O7 C62 C63 118.4(3) . . ?
C61 C62 C63 119.7(3) . . ?
C62 C63 C64 121.0(4) . . ?
C63 C64 C65 120.2(4) . . ?
C64 C65 C66 119.5(4) . . ?
C61 C66 C65 122.2(3) . . ?
Co1 N70 C71 121.5(2) . . ?
Co1 N70 C75 121.3(2) . . ?
C71 N70 C75 117.2(3) . . ?
N70 C71 C72 122.4(4) . . ?
C71 C72 C73 119.9(4) . . ?
C72 C73 C74 118.2(4) . . ?
C73 C74 C75 118.6(4) . . ?
N70 C75 C74 123.7(4) . . ?
Co1 N80 C81 121.7(2) . . ?
Co1 N80 C85 120.9(2) . . ?
C81 N80 C85 117.2(3) . . ?
N80 C81 C82 123.1(3) . . ?
C81 C82 C83 119.1(4) . . ?
C82 C83 C84 118.5(4) . . ?
C83 C84 C85 119.0(4) . . ?
N80 C85 C84 123.1(4) . . ?
C2S N1S C6S 121.7(4) . . ?
N1S C2S C3S 119.3(4) . . ?
C2S C3S C4S 118.5(4) . . ?
C3S C4S C5S 118.4(5) . . ?
C4S C5S C6S 124.3(4) . . ?
N1S C6S C5S 117.8(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.040(2) . ?
Co1 O3 2.045(2) . ?
Co1 O5 2.013(2) 3_665 ?
Co1 O6 2.057(2) 3_665 ?
Co1 N70 2.167(3) . ?
Co1 N80 2.202(3) . ?
O1 C22 1.367(4) . ?
O2 C20 1.301(4) . ?
O3 C30 1.291(4) . ?
O4 C40 1.351(4) . ?
O5 Co1 2.013(2) 3_665 ?
O5 C50 1.271(4) . ?
O6 Co1 2.058(2) 3_665 ?
O6 C60 1.301(4) . ?
O7 C62 1.360(4) . ?
C20 C21 1.491(5) . ?
C20 C31 1.395(5) . ?
C21 C22 1.411(5) . ?
C21 C26 1.406(5) . ?
C22 C23 1.395(5) . ?
C23 C24 1.368(5) . ?
C24 C25 1.392(5) . ?
C25 C26 1.368(5) . ?
C30 C31 1.400(5) . ?
C30 C42 1.500(5) . ?
C40 C41 1.412(5) . ?
C40 C42 1.416(5) . ?
C41 C43 1.384(5) . ?
C41 C50 1.502(5) . ?
C42 C44 1.404(5) . ?
C43 C45 1.394(5) . ?
C44 C45 1.381(5) . ?
C50 C51 1.419(5) . ?
C51 C60 1.394(5) . ?
C60 C61 1.498(5) . ?
C61 C62 1.418(5) . ?
C61 C66 1.399(5) . ?
C62 C63 1.396(5) . ?
C63 C64 1.369(5) . ?
C64 C65 1.386(5) . ?
C65 C66 1.377(5) . ?
N70 C71 1.348(5) . ?
N70 C75 1.329(5) . ?
C71 C72 1.367(6) . ?
C72 C73 1.382(6) . ?
C73 C74 1.373(6) . ?
C74 C75 1.382(6) . ?
N80 C81 1.341(4) . ?
N80 C85 1.339(4) . ?
C81 C82 1.368(5) . ?
C82 C83 1.382(5) . ?
C83 C84 1.374(5) . ?
C84 C85 1.375(5) . ?
N1S C2S 1.404(6) . ?
N1S C6S 1.332(6) . ?
C2S C3S 1.362(6) . ?
C3S C4S 1.376(6) . ?
C4S C5S 1.376(6) . ?
C5S C6S 1.309(6) . ?
